TY - CONF A1 - Baier, Jennifa A1 - Beck, Uwe A1 - Hidde, Gundula A1 - Hielscher, Stefan A1 - Lange, Thorid A1 - Mix, Renate T1 - Plasmagestützte Oberflächenfunktionalisierung von Polypropylen (PP) T2 - Teilnahmeunterlagen zum Workshop "Haftung durch Oberflächenfunktionalisierung" N2 - Polypropylen (PP) ist als Niedrigenergie-Polymer ohne nass- und plasmachemische Vorbehandlung weder haftfest zu beschichten noch verbundfest zu kleben. Typische Haft- bzw. Klebfestigkeiten liegen für die unbehandelte Polymeroberfläche bei maximal 0,5 MPa. Hinzu kommt, dass bei der Bestimmung von Haft- und Klebfestigkeiten der unmodifizierten Oberfläche mit großen Streuungen zu rechnen ist, die bezogen auf die Spannweite durchaus einem Faktor 5 entsprechen können. Generell besteht bei Prüfung der Haftfestigkeit mittels Stirnabzugsversuch und bei der Prüfung der Klebfestigkeit die Notwendigkeit eines statistisch validierten Herangehens. Hierzu sind zeitaufwändige Ein-Proben-Klebungen und -Prüfungen nur eingeschränkt geeignet. Zudem ist, insbesondere für geringe Haft- bzw. Klebfestigkeiten, ein querkraftfreies Prüfen Grundvoraussetzung. Im vorliegenden Beitrag werden verschiedenartige plasmagestützte Oberflächenfunktionalisierungen von PP sowie das Mehr-Proben-Konzept zur Klebung/Prüfung von bis zu acht Proben vorgestellt. Dazu werden ein BAM-Funktionsmuster einer Mehr-Proben-Kleb-Vorrichtung und eine kommerzielle analytische Zentrifuge zum Prüfen verwendet. T2 - 24. Workshop des Anwenderkreises Atmosphärendruckplasma "Haftung durch Oberflächenfunktionalisierung" CY - Erfurt, Germany DA - 11.11.2015 KW - Plasmamodifizierung KW - Polypropylen KW - Haftfestigkeit KW - Klebfestigkeit KW - Mehr-Proben-Kleben/-Prüfen PY - 2015 SP - 1 EP - 6 PB - Anwenderkreis Atmosphärendruckplasma CY - Jena AN - OPUS4-34838 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beck, Uwe A1 - Baier, Jennifa A1 - Hidde, Gundula A1 - Hielscher, Stefan A1 - Kittler-Packmor, Kai A1 - Lange, Thorid A1 - Mix, Renate A1 - Weise, Matthias T1 - Multiple-sample approach: reliable ranking and validated statistics of bonding and adhesive strength JF - Dispersion Letters N2 - Bonding strength of adhesive-bonded joints and adhesive strength of coatings have been exclusively determined in single-sample tests using a tensile testing machine. Necessarily, the single-sample approach was also applied to the corresponding bonding procedure. As a consequence, reliability and reproducibility of results were restricted. By applying the newly introduced centrifuge technology, the multiple-sample approach was realized for simultaneous tensile testing of up to eight samples under identical conditions without any disturbing shear-force effects. In order to introduce the multiple-sample approach into the bonding procedure, a hydraulic bonding set-up was developed which enables identical bonding pressure also for slightly different heights of sample assemblies. Both sample approaches were compared for various application examples: ranking of different classes of adhesives, validated statistics of adhesive-bonded joints using one particular adhesive and effects of cleaning and plasma-treatment on the adhesive strength of coatings. The investigated systems included glass, metals and polymer substrates, different adhesives, metallic and dielectric coatings on polymers. KW - Bonding strength KW - Adhesive strength KW - Multi-sample approach KW - Centrifuge technology PY - 2014 SN - 978-3-944261-28-7 SN - 978-3-944261-36-2 SN - 978-3-944261-52-2 VL - 5 SP - 1 EP - 5 AN - OPUS4-31310 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Baier, Jennifa A1 - Hidde, Gundula A1 - Hielscher, Stefan A1 - Kittler-Packmor, Kai A1 - Lange, Thorid A1 - Mix, Renate A1 - Weise, Matthias T1 - Multiple-sample approach: reliable ranking and validated statistics of bonding and adhesive strength T2 - EURADH 2014 - 10th European Adhesion Conference (Proceedings) N2 - Bonding strength of adhesive-bonded joints and adhesive strength of coatings have been exclusively determined in single-sample tests using a tensile testing machine. Necessarily, the single-sample approach was also applied to the corresponding bonding procedure. As a consequence, reliability and reproducibility of results were restricted. By applying the newly introduced centrifuge technology, the multiple-sample approach was realized for simultaneous tensile testing of up to eight samples under identical conditions without any disturbing shear-force effects. In order to introduce the multiple-sample approach into the bonding procedure, a hydraulic bonding set-up was developed which enables identical bonding pressure also for slightly different heights of sample assemblies. Both sample approaches were compared for various application examples: ranking of different classes of adhesives, validated statistics of adhesive-bonded joints using one particular adhesive and effects of cleaning and plasma-treatment on the adhesive strength of coatings. The investigated systems included glass, metals and polymer substrates, different adhesives, metallic and dielectric coatings on polymers. T2 - EURADH 2014 - 10th European Adhesion Conference CY - Alicante, Spain DA - 22.04.2014 KW - Bonding strength KW - Adhesive strength KW - Multi-sample approach KW - Centrifuge technology PY - 2014 SN - 978-84-616-9067-1 SN - 84-616-9067-2 SP - Paper 49, 211 EP - 214 AN - OPUS4-31309 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mix, Renate A1 - Friedrich, Jörg Florian A1 - Neubert, Dietmar A1 - Inagaki, N. T1 - Response of linear, branched or crosslinked polyethylene structures on the attack of oxygen plasma JF - Plasma chemistry and plasma processing N2 - Linear, branched and crosslinked polyethylenes (PE) were exposed to the low-pressure oxygen plasma for 2–120 s. In the following the samples were washed with solvents to remove low-molecular weight oxidized material and to excavate the subjacent polymer structure for microscopic characterization. X-ray photoelectron spectroscopy (XPS) measurements provided information about changes in elemental composition and chemical structure of PE after plasma exposure and washing. The calculation of the concentration of tertiary C atoms using XPS data was a measure of branches and crosslinking in the polymer before and after exposure to oxygen plasma. Linear PE was most sensitive towards oxygen plasma and showed the highest concentration in tertiary C atoms after plasma exposure. On the other hand branched PE types, which possess originally more tertiary carbon atoms, have lost two-third of them after 2 s oxygen plasma exposure. Branched PE show also topological changes at their surface as detected by atomic force microscopy. Differential scanning calorimetry measurements confirmed strong changes in crystallinity and molecular orientation of linear PE already after 120 s exposure to the oxygen plasma interpreted as amorphization. These effects should be interpreted as result of crosslinking caused by the recombination of dangling bond sites. KW - Linear and branched polyethylene KW - Oxygen plasma KW - Functionalization KW - Crosslinking PY - 2014 UR - http://link.springer.com/article/10.1007%2Fs11090-014-9558-9/fulltext.html DO - https://doi.org/10.1007/s11090-014-9558-9 SN - 0272-4324 VL - 34 IS - 5 SP - 1199 EP - 1218 PB - Plenum Publ. Corp. CY - New York, NY, USA AN - OPUS4-30741 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kricheldorf, H.R. A1 - Mix, Renate A1 - Weidner, Steffen T1 - Poly(ester urethane)s derived from lactide, isosorbide, terephthalic acidm abd various diisocyanates JF - Journal of polymer science A, polymer chemistry N2 - Isosorbide-initiated oligomerizations of ʟ-lactide were preformed in bulk using SnCl2 as catalyst. The resulting telechelic OH-terminated oligoesters were in situ subjected to simultaneous polycondensation and polyaddition with mixtures of terephthaloyl chloride and diisocyanates. Most polymerizations were conducted with 4,4'-diisocyanatodiphenyl methane and 2,4-diisocyanato toluene. The consequences of excess diisocyanate and four different catalysts were studied. The isosorbide/lactide ratio and the terephthalic acid/diisocyanate ratio were varied. Number average molecular weights up to 15 kDa with polydispersities around 3–5 were obtained. Depending on the chemical structure of the copolyester and on the feed ratio, incorporation of urethane groups may reduce or enhance the glass-transition temperature, but the thermal stability decreases dramatically regardless of composition. KW - Cyclization KW - Isosorbide KW - Lactide KW - Polyaddition KW - Polycondensation KW - Polyesters KW - Polyurethanes PY - 2014 DO - https://doi.org/10.1002/pola.27069 SN - 0360-6376 SN - 0887-624X VL - 52 IS - 6 SP - 867 EP - 875 PB - Wiley CY - Hoboken, NJ AN - OPUS4-30299 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Mix, Renate A1 - Friedrich, Jörg Florian A1 - Inagaki, N. ED - Thomas, M. ED - Mittal, K.L. T1 - Permanence of functional groups at polyolefin surfaces introduced by dielectric barrier discharge pretreatment in presence of aerosols T2 - Atmospheric pressure plasma treatment of polymers N2 - A convenient way to overcome the chemical inertness of polyolefin surfaces is to expose them to the atmospheric air plasma of a dielectric barrier discharge (DBD). To improve the efficiency in formation of polar groups at the polyolefin surface, different liquids such as water and ethanol were sprayed as aerosol into the plasma zone between the powered electrode and the polyolefin surface. Both sprayed liquids as well as the polyolefin surface were simultaneously activated; thus, the formation of different functional groups at the polyolefin surface was realized. The type of aerosol-sprayed additive, exposure time, power etc. have been found to determine the efficiency with respect to introduction of polar groups. KW - PE KW - PP KW - Surface modification KW - Aerosol-assisted DBD PY - 2013 SN - 978-1-118-59621-0 DO - https://doi.org/10.1002/9781118747308.ch4 N1 - Serientitel: Adhesion and Adhesives: Fundamental and applied aspects – Series title: Adhesion and Adhesives: Fundamental and applied aspects IS - Part 1 / Chapter 4 SP - 131 EP - 156 PB - Wiley AN - OPUS4-28657 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Friedrich, Jörg Florian A1 - Mix, Renate T1 - Combination of plasma-chemical and wet-chemical processes - a simple way to optimize interfaces in metal-polymer composites for maximal adhesion T2 - ISPC 21 - 21st International Symposium on Plasma Chemistry N2 - Different surface treatments of polypropylene (PP) were tested to improve the peel strength of aluminium-PP systems. Plasma exposure followed by chemical grafting of spacers with -SiOH endgroups and thin adhesion promoting layers deposited by aerosol-assisted DBD using aqu. solutions of classic polymers were compared. Both methods were effective, however, –SiOH terminated spacers effected no peeling also after ageing. T2 - ISPC 21 - 21st International Symposium on Plasma Chemistry CY - Cairns, QLD, Australia DA - 2013-08-02 KW - Adhesion polypropylene-aluminium KW - Tailored interface structures KW - Aerosol-assisted DBD PY - 2013 UR - http://www.ispc-conference.org/ispcproc/ispc21/ID549.pdf SP - Paper 549, 1 EP - 4 AN - OPUS4-28661 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fahmy, A. A1 - Mix, Renate A1 - Schönhals, Andreas A1 - Friedrich, Jörg Florian T1 - Structure of plasma-deposited copolymer films prepared from acrylic acid and styrene: Part II variation of the comonomer ratio JF - Plasma processes and polymers N2 - Copolymers of acrylic acid and styrene (AA/S) were prepared by pulsed plasma deposition technique. Their structure–property relationships were studied in dependence on the comonomer ratio. Both, the regularity of the structure and the composition of the thin copolymer films were investigated by bulk-sensitive (dielectric spectroscopy, FTIR, and differential scanning calorimetry) as well as surface-sensitive methods such as X-ray photoelectron spectroscopy (XPS). For an unambiguous identification of the functionality of the deposited films the COOH groups were estimated by derivatization with trifluoroethanol and subsequent XPS measurement as well as by the quantitative analysis of the FTIR data. As a result, the concentration of COOH groups on the surface and in the bulk is increasing with the fraction of AA in precursor mixture in a non-monotonous way but similar to the dependence obtained by conventional free radical polymerization. KW - Acrylic acid-styrene copolymer KW - Bulk properties KW - Dielectric properties KW - Plasma polymerization KW - Surface functionalization PY - 2013 DO - https://doi.org/10.1002/ppap.201200110 SN - 1612-8850 SN - 1612-8869 VL - 10 IS - 9 SP - 750 EP - 760 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-29096 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mix, Renate A1 - Hielscher, Stefan A1 - Beck, Uwe A1 - Friedrich, Jörg F. T1 - Adhesion Promotion in Aluminium Polypropylene Composites Measured by Peel test and Centrifuge technology T2 - 19th International Vacuum Congress (IVC-19) T2 - 19th International Vacuum Congress (IVC-19) CY - Paris, France DA - 2013-09-09 PY - 2013 AN - OPUS4-29552 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Mix, Renate A1 - Yin, Huajie A1 - Friedrich, Jörg Florian ED - Gutowski, W. ED - Dodiuk, H. T1 - Aerosol-based DBD - A simple way to provide polymers with functional groups for adhesion promotion T2 - Recent advances in adhesion science and technology in honor of Dr. Kash Mittal N2 - Polypropylene (PP) foils were exposed to the plasma of an atmospheric dielectric barrier discharge (DBD) in presence of different aerosols. Pure liquids such as water, ethanol, and 1/1 mixtures ethanol/water (v/v) or aqueous Solutions of acetic acid, poly(acrylic acid), poly(vinyl alcohol), and ethylene glycolpoly(vinyl alcohol) copolymer were introduced into the DBD. Surface composition, the number of functional groups per 100 C atoms, and water contact angles were correlated with the energy density of DBD plasma exposure. The wettability of the treated surfaces was investigated for different storage times. Peel strength of the thermally deposited aluminum layer to modified polymer surfaces revealed that the aerosol introduction strongly improves the adhesion between aluminum and polypropylene. KW - Aerosol-assisted DBD KW - Functional groups KW - Surface modification PY - 2013 SN - 978-90-04-20173-6 SN - 978-90-04-20174-3 SP - Chapter 8, 155 EP - 170 PB - CRC Press AN - OPUS4-30035 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -